تفاعل #1950485

ord-61a057739ad14201a40aa486ccf675ea

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture is refluxed for 20 hours
  2. 2
    أخرىthe solvent removed in vacuo
  3. 3
    workup.ADDITIONTo the residue is added water
  4. 4
    استخلاصthe mixture is extracted with ether
  5. 5
    غسيلThe ether extracts are washed with 10% potassium carbonate and with water
  6. 6
    تجفيفdried (MgSO4)
  7. 7
    أخرىEvaporation of the solvent under vacuum
  8. 8
    أخرىgives a tan oil
  9. 9
    ترشيحfiltered through a column of silica gel
  10. 10
    أخرىRemoval of the solvent from the second 200 ml

الإجراء التجريبي

To a solution of 4.93 g of 3,4,5-trichlorophenol and 1.19 g of sodium methoxide in 40 ml of methanol is added 7.11 g of methyl α-bromo-α-[p-(p-chlorophenoxy)phenyl]acetate in 10 ml of benzene and 50 mg of potassium iodide. The mixture is refluxed for 20 hours and the solvent removed in vacuo. To the residue is added water and the mixture is extracted with ether. The ether extracts are washed with 10% potassium carbonate and with water and dried (MgSO4). Evaporation of the solvent under vacuum gives a tan oil. The oil is dissolved in chloroform and filtered through a column of silica gel. Removal of the solvent from the second 200 ml cut gives the product as a tan oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04168385uspto-grants-1979_09